CN113092540A - Novel high-sensitivity micro-humidity sensor and preparation method thereof - Google Patents
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- CN113092540A CN113092540A CN202110312310.7A CN202110312310A CN113092540A CN 113092540 A CN113092540 A CN 113092540A CN 202110312310 A CN202110312310 A CN 202110312310A CN 113092540 A CN113092540 A CN 113092540A
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- 238000005516 engineering process Methods 0.000 claims abstract description 7
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- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 9
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
- G01N27/125—Composition of the body, e.g. the composition of its sensitive layer
- G01N27/126—Composition of the body, e.g. the composition of its sensitive layer comprising organic polymers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K26/00—Working by laser beam, e.g. welding, cutting or boring
- B23K26/36—Removing material
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
- G01N27/125—Composition of the body, e.g. the composition of its sensitive layer
- G01N27/127—Composition of the body, e.g. the composition of its sensitive layer comprising nanoparticles
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
- G01N27/128—Microapparatus
Abstract
The invention discloses a novel high-sensitivity micro-humidity sensor and a preparation method thereof, belonging to the technical field of humidity sensors, wherein the device is formed by assembling two layers of PEGDA/PI films; the PEGDA/PI film is prepared by adhering PEGDA hydrogel on a PI substrate, introducing a micro-nano structure on the surface of the PEGDA by a femtosecond laser direct writing technology, adding a layer of carbon nano film on the PEGDA, and dripping the silver paste on two sides of a device for connecting electrodes. The invention adopts hydrogel as a humidity sensitive material to prepare the sensor with small volume and high sensitivity and a precise PEGDA/PI film with micron-scale size, and is beneficial to the miniaturization and integration of the sensor. The high-sensitivity miniature humidity sensor provided by the invention has a fine structure, the water absorption expansion and contraction capacity of the PEGDA hydrogel with the microstructure and the femtosecond laser direct writing scanning interval present an approximately linear relationship, and the size of the micro-nano structure adjusts and controls the photocrosslinking degree by changing the laser processing parameters, so that the expansion/contraction rate of the hydrogel is adjusted and controlled.
Description
Technical Field
The invention belongs to the technical field of humidity sensors, and particularly relates to a novel high-sensitivity micro-humidity sensor and a preparation method thereof.
Background
The humidity sensor has wide application in the fields of meteorological monitoring, industrial production, agricultural planting, aerospace, medical treatment and the like, and is an important sensor. Humidity sensors can be classified into two categories, water molecule affinity type and non-water molecule affinity type, according to the working principle. The working principle of the water molecule affinity type humidity sensor is that the characteristics of the humidity sensor are changed in the processes of water molecule adsorption and water molecule desorption of hydrophilic substances, so that the humidity is measured. The water molecule affinity type humidity sensor has small size, and the test circuit has simple structure and is very suitable for integration.
The hydrogel as a hydrophilic soft material has biocompatibility and good flexibility, and can be applied to the fields of pressure sensors, strain sensors, brakes and the like. In addition, the hydrogel has excellent mechanical properties, can bear large mechanical deformation and distortion, and does not reduce the sensing performance due to severe mechanical deformation. Hydrogels are therefore considered to be an ideal choice for wetness sensors.
The device prepared by the traditional manufacturing process is large in size, and with the development of the Internet of things, the sensor with single variable and single function cannot meet the requirement. Integration and array of various sensors are one of solutions. Therefore, the sensor is required to be designed in a micro structure, and the volume of the sensor unit is reduced to adapt and promote the development and the practicability of the integrated sensor. There is still a need for a high performance humidity sensor with high sensitivity, low power consumption and micro-size.
Disclosure of Invention
In order to overcome the defects of larger size, single function and the like of a device prepared by the traditional manufacturing process in the prior art, the invention provides a novel high-sensitivity micro-humidity sensor and a preparation method thereof. The femtosecond laser two-photon polymerization is utilized to process micron-level fine structures on the surface layer of the hydrogel, so that the contact area of the device and the ambient air is increased, and the sensitivity and the integration level of the humidity sensor are improved.
The invention is realized by the following technical scheme:
a novel high-sensitivity micro-humidity sensor is formed by assembling two layers of PEGDA/PI films; the PEGDA/PI film is prepared by adhering PEGDA hydrogel on a PI substrate, introducing a micro-nano structure on the surface of the PEGDA by a femtosecond laser direct writing technology, adding a layer of carbon nano film on the PEGDA, and dripping the silver paste on two sides of a device for connecting electrodes.
Preferably, the thickness of the carbon nano-film is in the range of 30-50 nm.
A preparation method of a novel high-sensitivity micro-humidity sensor comprises the following specific steps:
the method comprises the following steps: the surface roughness of the PI (polyimide) thin-layer substrate is increased through acid-base treatment, the adhesive force is improved, and the apparent quality and the inherent mechanical property are not influenced; and uniformly coating a layer of PEGDA hydrogel on the treated PI substrate.
Step two: generating a TXT data document consisting of coordinate points of a structure to be processed by using a C # language in Visual Studio software, drawing a designed three-dimensional structure by using data, and preparing the designed structure on PEGDA hydrogel by using a femtosecond laser direct writing system in a two-photon polymerization mode;
step three: mixing ethanol and water in a volume ratio of 2:1 to prepare a developing solution, completely immersing the structure into the developing solution, and removing the part which is not cured by the femtosecond laser focal spot to obtain the required structure;
step four: spraying a layer of carbon nanotube film on the prepared PEGDA, and then placing the PEGDA on a heating platform for curing;
step five: silver paste is dripped on one side of the integral structure for connecting electrodes;
step six: repeating the steps to obtain two same structures which are assembled together in a facing way to form the sensor.
Preferably, the PEGDA hydrogel in step one has a thickness of 1-5 μm.
Preferably, the acid-base treatment in the step one is to treat the PI (polyimide) substrate with oxalic acid solution, NaOH solution, and desalted water, respectively.
Preferably, in the second step, the femtosecond laser direct writing system adopts laser with a central wavelength of 800nm, a laser pulse width of 100fs, a repetition frequency of 80GHz, a focused laser focal spot diameter of 700nm, a femtosecond laser exposure power of 15mW, and an exposure time of 500 μ s.
Preferably, the temperature for curing the carbon nanotubes in the fourth step is 80 ℃. And the hydrogel is not affected by temperature.
Compared with the prior art, the invention has the following advantages:
1. the invention adopts hydrogel as a humidity sensitive material to prepare the sensor with small volume and high sensitivity. By adjusting the program, a precise PEGDA/PI film with the size of micron can be prepared, and the miniaturization and the integration of the sensor are facilitated.
2. The invention adopts the femtosecond laser two-photon direct writing technology and simultaneously cooperates with the programming software to control the precise deflection of the scanning galvanometer, thereby realizing that any three-dimensional complex micro-nano structure with high precision and high design degree can be obtained on the PEGDA.
3. The introduction of the microstructure increases the contact area of the device and the ambient air, and is beneficial to the adsorption and desorption of the humidity sensor to the surrounding water molecules in the water vapor environment, thereby improving the sensitivity of the sensor.
4. The high-sensitivity miniature humidity sensor provided by the invention has a fine structure, the water absorption (water loss) expansion (contraction) capability of the structure of the PEGDA hydrogel and the femtosecond laser direct writing scanning interval show an approximately linear relationship, and the size of the micro-nano structure can adjust and control the photocrosslinking degree by changing the laser processing parameters, so that the expansion/contraction rate of the hydrogel is adjusted and controlled.
Drawings
In order to more clearly illustrate the detailed description of the invention or the technical solutions in the prior art, the drawings that are needed in the detailed description of the invention or the prior art will be briefly described below. Throughout the drawings, like elements or portions are generally identified by like reference numerals. In the drawings, elements or portions are not necessarily drawn to scale.
FIG. 1 is a schematic structural diagram of a novel high-sensitivity micro humidity sensor according to the present invention;
FIG. 2 is a schematic diagram of a femtosecond laser processing device for three-dimensional parametric patterns of micro-nano structures in the invention;
fig. 3 is a three-dimensional schematic view of a PEGDA hydrogel having microstructures according to the present invention.
Detailed Description
The following embodiments are only used for illustrating the technical solutions of the present invention more clearly, and therefore, the following embodiments are only used as examples, and the protection scope of the present invention is not limited thereby.
It is to be noted that, unless otherwise specified, technical or scientific terms used herein shall have the ordinary meaning as understood by those skilled in the art to which the invention pertains.
Example 1
The embodiment provides a novel high-sensitivity micro humidity sensor, as shown in fig. 1, the device is formed by assembling two layers of PEGDA/PI films; the PEGDA/PI film is prepared by adhering PEGDA hydrogel on a PI substrate, introducing a micro-nano structure on the surface of the PEGDA by a femtosecond laser direct writing technology, adding a layer of carbon nano film on the PEGDA, and dripping the silver paste on two sides of a device for connecting electrodes. The thickness range of the carbon nano film is 30-50 nm.
Example 2
To facilitate understanding of the present embodiment, first, a detailed description is given of a method for manufacturing a novel high-sensitivity micro humidity sensor according to an embodiment of the present invention. The overall structure of the device is shown in fig. 1, the PEGDA is used as a humidity sensitive material to convert the humidity in the environment into a usable signal, the PEGDA hydrogel structure is photocured by combining computer programming and a femtosecond laser two-photon polymerization direct writing technology, a pre-designed three-dimensional micro-nano structure is obtained, and a layer of carbon nano tubes is added. Finally, the structure is repeatedly prepared, is just assembled together and is externally connected with an electrode, and the novel high-sensitivity micro-humidity sensor is prepared.
A preparation method of a novel high-sensitivity micro-humidity sensor comprises the following specific steps:
step 1: the PI (polyimide) substrate is treated by oxalic acid solution, NaOH and desalted water, and the PI is not resistant to strong alkali and is contacted with the NaOH to be equivalent to etching the surface of the PI substrate, so that the roughness of the surface of the PI substrate is increased, the adhesive force of the PI substrate is greatly improved, and the apparent quality and the inherent mechanical property of the PI substrate are not influenced. And after acid and alkali treatment, uniformly coating a layer of PEGDA hydrogel on a PI substrate by a spin coater. The PEGDA is a polymer material with quick and obvious response to the environmental humidity, and PI and PEGDA are biocompatible, safe and nontoxic.
Step 2: generating a TXT data document consisting of structure coordinate points by using a C # language in Visual Studio software, drawing a designed three-dimensional structure by data, and preparing the designed structure on PEGDA hydrogel by using a femtosecond laser direct writing system in a two-photon polymerization mode. The femtosecond laser direct writing system is shown in fig. 2.
And step 3: ethanol and water were mixed in a 2:1 volume ratio in a petri dish to prepare a developer solution, and the structure was completely immersed in the developer solution to remove the portions that were not solidified by the femtosecond laser focal spot, resulting in the desired structure (fig. 3).
And 4, step 4: a layer of carbon nanotubes is sprayed on the prepared PEGDA hydrogel and then placed on a heating platform to be cured at a temperature of 80 ℃.
And 5: silver paste was drop coated on one side of the monolithic structure to serve as an electrode.
Step 6: two layers of PEGDA hydrogel/PI with micro-nano structures are adopted to be assembled into a hydrogel miniature sensitive humidity sensor.
In this embodiment, the femtosecond laser direct writing system adopts a laser with a central wavelength of 800nm, a pulse width of 120fs, and a repetition frequency of 80 GHz. Laser generated by the femtosecond laser oscillator 1 firstly passes through the lens 2 with a short focal length, the optical gate 3 and the lens 4 with a long focal length, reaches a beam expanding effect, then enters the two-dimensional scanning galvanometer 6 through the high reflecting mirror 5, and is combined with the following one-dimensional piezoelectric platform to realize three-dimensional movement of the light beam. After scanning the galvanometer, the optical scanning device enters a 4f lens system and consists of two plano- convex lenses 7 and 8 with the same focal length. Finally, the light beam passes through a high-reflection mirror 9 to be vertically downward and is tightly focused in the PEGDA on the one-dimensional piezoelectric platform 11 through a high-numerical-aperture oil lens 10. The precise deflection of the scanning galvanometer is controlled by programming software, so that the three-dimensional parametric pattern femtosecond laser processing of the PEGDA hydrogel is realized. The CCD camera is also connected with a computer to observe and adjust the processing process in real time. The system has the processing precision of about 100 nm.
In this example, the novel highly sensitive micro humidity sensor employs the following principle: the PEGDA hydrogel can regulate the absorption or release of water molecules, and realize the regulation of expansion and contraction. When the hydrogel absorbs water and expands, the upper and lower layers of carbon nanotubes are extruded, so that the contact area is enlarged, and the resistance of the sensor is reduced. Similarly, when the hydrogel releases water molecules, the volume shrinks, the contact area of the carbon nano tube becomes small, and the resistance becomes large. In addition, the femtosecond laser two-photon polymerization direct writing technology is introduced, a fine micro-nano structure is prepared on the hydrogel, the contact area of the carbon nano tube is increased, the size of the micro-nano structure can be adjusted and controlled through changing laser processing parameters, and the expansion/shrinkage rate of the hydrogel is further adjusted and controlled.
In the present example, the introduction of the microstructure in the novel high-sensitivity micro humidity sensor increases the contact area of PEGDA and air, so that the PEGDA can adsorb and desorb water vapor more effectively; on the other hand, the microstructure can also increase the contact area of the upper PEGDA/PI film and the lower PEGDA/PI film, so that the sensitivity of the device is improved. In addition, the preparation of the microstructures is based on femtosecond laser two-photon polymerization, so that the size and the morphology of the microstructures are customizable.
The preferred embodiments of the present invention have been described in detail with reference to the accompanying drawings, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications can be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that the various technical features described in the above embodiments can be combined in any suitable manner without contradiction, and the invention is not described in any way for the possible combinations in order to avoid unnecessary repetition.
In addition, any combination of the various embodiments of the present invention is also possible, and the same should be considered as the disclosure of the present invention as long as it does not depart from the spirit of the present invention.
Claims (7)
1. A novel high-sensitivity micro-humidity sensor is characterized in that the device is formed by assembling two layers of PEGDA/PI films; the PEGDA/PI film is prepared by adhering PEGDA hydrogel on a PI substrate, introducing a micro-nano structure on the surface of the PEGDA by a femtosecond laser direct writing technology, adding a layer of carbon nano film on the PEGDA, and dripping the silver paste on two sides of a device for connecting electrodes.
2. The novel highly sensitive micro humidity sensor as claimed in claim 1, wherein the thickness of the carbon nano-film is in the range of 30-50 nm.
3. The method for preparing a novel high-sensitivity micro-humidity sensor according to claim 1, comprising the following steps:
the method comprises the following steps: the PI thin-layer substrate is subjected to acid-base treatment, so that the surface roughness is increased, the adhesive force is improved, and the apparent mass and the inherent mechanical property are not influenced; uniformly coating a layer of PEGDA hydrogel on the treated PI substrate;
step two: generating a TXT data document consisting of coordinate points of a structure to be processed by using a C # language in Visual Studio software, drawing a designed three-dimensional structure by using data, and preparing the designed structure on PEGDA hydrogel by using a femtosecond laser direct writing system in a two-photon polymerization mode;
step three: mixing ethanol and water in a volume ratio of 2:1 to prepare a developing solution, completely immersing the structure into the developing solution, and removing the part which is not cured by the femtosecond laser focal spot to obtain the required structure;
step four: spraying a layer of carbon nanotube film on the prepared PEGDA, and then placing the PEGDA on a heating platform for curing;
step five: silver paste is dripped on one side of the integral structure for connecting electrodes;
step six: repeating the steps to obtain two same structures which are assembled together in a facing way to form the sensor.
4. The novel highly sensitive micro-humidity sensor as claimed in claim 3, wherein the PEGDA hydrogel in step one has a thickness of 1-5 μm.
5. The novel high-sensitivity micro-humidity sensor as claimed in claim 3, wherein the acid-base treatment in the first step is to treat the PI substrate with oxalic acid solution, NaOH solution and desalted water respectively.
6. The novel high-sensitivity micro-humidity sensor as claimed in claim 3, wherein in step two, the femtosecond laser direct writing system adopts a laser center wavelength of 800nm, a laser pulse width of 100fs, a repetition frequency of 80GHz, a focused laser focal spot diameter of 700nm, a femtosecond laser exposure power of 15mW, and an exposure time of 500 μ s.
7. The novel highly sensitive micro humidity sensor of claim 3, wherein the temperature for curing the carbon nanotubes in step four is 80 ℃.
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